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ChemicalBook CAS DataBase List 5-(Trifluoromethyl)-2-pyridinemethanamine
164341-39-3

5-(Trifluoromethyl)-2-pyridinemethanamine synthesis

5synthesis methods
80194-70-3 Synthesis
2-Cyano-3-chloro-5-(trifluoromethyl)-pyridine

80194-70-3
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Yield: 38%

Reaction Conditions:

with 5%-palladium/activated carbon;hydrogen in ethanol;water at 60; under 15001.5 - 18751.9 Torr; for 25 h;Autoclave;

Steps:

1 Comparative example 1
Into a 500mL autoclave, 20.85g (0.1mol, 99%, 1.0eq) of 2-cyano-3-chloro-5-trifluoromethylpyridine was sequentially added,5% palladium-carbon wet base 4.55g (54.5% water) and 170g ethanol.Replace the system with nitrogen three times and hydrogen three times,Pass hydrogen to the pressure in the kettle to 2.0-2.5Mpa,The temperature is controlled at 60 and the reaction is kept for about 20h without pressure lossContinue to incubate and react for 5 hours, take samples for HPLC control,The system is very complicated,The raw material remains about 5%, 2-aminomethyl-5-trifluoromethylpyridine is about 38%,One of the main impurities is about 40% of the product (secondary amine) obtained by removing one molecule of ammonia from two molecules of 2-aminomethyl-5-trifluoromethylpyridine.No post-processing was performed.

References:

Dalian Jiu Xin Fine Chemical Co., Ltd.;Wang Junchun;Wang Rongliang;Lv Chao;Wang Yanbo;Cong Xiaoqiang CN111170932, 2020, A Location in patent:Paragraph 0045-0046

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